Preparation method and purification method of azacyclo-sulfide

Abstract

The invention relates to the technical field of organic synthesis, in particular to a preparation method of azacyclo-sulfide and a purification method of same. The preparation method comprises the steps of raw material extraction, substrate expansion, nucleophilic preparation, oxidation modification, vibration, standing and purification. A reaction tank comprises a tank body, a reaction vessel anda burette; a plurality of layers of reaction vessels are arranged in the tank body; the burette pipeline comprises a titration disc and a shunt pipe; because the dispersion degrees of the substratesin the mixed solution are different and the speed of adding the substrates into the reaction tank is changed, the purity effect of the required azacyclo-sulfide extraction can be influenced; therefore, according to the invention, the reaction vessel and the titration disc are correspondingly arranged in the reaction tank; the reaction vessel is provided with the inclined reaction tank, the speed of a substrate solution entering the titration disc is balanced by matching with the shunt pipe inclined to the titration disc, and the servo motor drives the inclined reaction tank to rotate, so thatthe substrate added into the reaction vessel uniformly covers the surface of the reaction vessel, and the preparation purity of the azacyclo-sulfide is improved.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of nitrogen heterocyclic sulfides and a purification method thereof. Background technique [0002] Nitrogen-containing heterocyclic compounds have many applications in medicine, materials, catalysis, etc. More than half of the drugs used by people are nitrogen-containing heterocyclic compounds; there are harsh conditions and complicated operations in the process of synthesizing such compounds. , low reaction efficiency and other shortcomings, so it is of great significance to study the method of synthesizing such heterocyclic compounds with high selectivity and high yield; since organosulfur compounds are widely found in organic synthetic chemistry, medicinal chemistry, etc., they are valuable synthetic The approach to sulfur-heterobonding has also become an important area of ​​concern for chemists. [0003] In the prior art, there are also some te...

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Problems solved by technology

[0002] Nitrogen-containing heterocyclic compounds have many applications in medicine, materials, catalysis, etc. More than half of the drugs used by people are nitrogen-containing heterocyclic compounds; there are harsh conditions and complicated operations in the process of synthesizing such compounds. , low reaction efficiency and other shortcomings, so it is of great significance to study the method of synthesizing such heterocyclic compounds with high selectivity and high yield; since organosulfur compounds are widely found in organic synthetic chemistry, medicinal chemistry, etc., they are valuable synthetic The approach to sulfur-heterobonds has also become an important area of ​​concern for chemists

[0003] In the prior art, there are also some technical solutions about the preparation method and purification method for the synthesis of nitrogen heterocyclic sulfides. For example, a Chinese patent with application number 2017110032623 discloses a preparation method for the synthesis of nitrogen heterocyclic sulfides and Purification and purification method, the steps include: using N-pyridylpyrrole or N-pyridylindole and disulfide as substrate, using dimethyl sulfoxide as solvent, under the catalysis of transition metal copper salt and the action of ligand, In the air environment, the crude product was obtained by heating and reacting, then, the crude product was filtered and the solvent was removed to obtain the residue; the residue was subjected to silica gel column chromatography, washed with the eluent, and the effluent was collected; combined with For the effluent of the product, the combined effluent is concentrated to remove the solvent, and finally the target product is obtained by vacuum drying; the technological process in this technical scheme is simple, the cost is low, and the yield is high; but the nitrogen heterocyclic sulfide in this technical scheme During the preparation process, the reaction of the nitrogen heterocycle and the sulfide functional group failed to effectively control its uniform synthesis effect, which reduced the concentration uniformity of the synthesis, which in turn increased the problems in the purification process

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